CN108517206A - A kind of preparation method of nano zine oxide core-shell quanta dots - Google Patents
A kind of preparation method of nano zine oxide core-shell quanta dots Download PDFInfo
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- CN108517206A CN108517206A CN201810472339.XA CN201810472339A CN108517206A CN 108517206 A CN108517206 A CN 108517206A CN 201810472339 A CN201810472339 A CN 201810472339A CN 108517206 A CN108517206 A CN 108517206A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
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- C—CHEMISTRY; METALLURGY
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/59—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing silicon
- C09K11/592—Chalcogenides
- C09K11/595—Chalcogenides with zinc or cadmium
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Abstract
The present invention is a kind of preparation method of nano zine oxide core-shell quanta dots, the specific steps are：Prepare zinc acetate solution, sodium hydroxide solution；Stirred in water bath by zinc acetate solution at 55 DEG C 60 DEG C dissolves；Stirred in water bath by sodium hydroxide solution at 50 DEG C dissolves；Zinc acetate solution is cooled to 50 DEG C of water-baths, dispersant is added, 20 25min is stirred, sodium hydroxide solution is then added, reacts 15min in 50 DEG C of water-baths, obtains nano oxidized zinc solution；It pipettes in concentrated ammonia liquor to ethanol solution and is diluted, ultrasonic mixing is uniform, obtains ammonium hydroxide dilution；Nano oxidized zinc solution obtained is cooled to 37 DEG C, water, ethyl orthosilicate, ammonium hydroxide dilution are added dropwise in stirring, 37 DEG C are stirred to react 60 70min, nano zine oxide core-shell quanta dots solution are made, and in 4 DEG C of preservations.The ultraviolet shielded effect of Zinc oxide quantum dot and the transparency prepared by the present invention is good, has application prospect.
Description
Technical field
The present invention relates to quantum dot preparation field more particularly to a kind of preparation methods of nano zine oxide core-shell quanta dots.
Background technology
Zinc oxide is a kind of II-VI race's wide bandgap semiconductor oxide, and nano zine oxide is had by its quantum size
Unique photoelectric characteristic, the energy gap with 3.37eV at normal temperatures, exciton binding energy is up to 60meV, becomes half
The material of great development prospect in conductor material.For other opposite quantum dots, nano zine oxide has nontoxic physical property,
Research based on nano zine oxide quantum dot rapidly becomes hot spot.
But the fluorescence of Zinc oxide quantum dot nevertheless suffers from the influence of various factors, as pH value, temperature, different metal sun from
Son and different anions etc., it is steady that influence of these factors of system research to fluorescence effectively further can probe into quantum dot
Application range that is qualitative and expanding nano material optical property is provided fundamental basis.
Invention content
The present invention is directed to study being synthetically prepared for Zinc oxide quantum dot, and provide a kind of nano zine oxide core-shell quanta dots
Preparation method.
The present invention to achieve the above object, using following technical scheme：
A kind of preparation method of nano zine oxide core-shell quanta dots, the specific steps are：
The preparation of S1, nano oxidized zinc solution
It weighs Zinc diacetate dihydrate to be dissolved in solvent, is configured to the zinc acetate solution of a concentration of 0.1mol/L, weighs hydrogen-oxygen
Change sodium to be dissolved in solvent, is configured to the sodium hydroxide solution of a concentration of 0.1mol/L；
Stirred in water bath by prepared zinc acetate solution at 55 DEG C -60 DEG C dissolves 30-40min；
Stirred in water bath by prepared sodium hydroxide solution at 50 DEG C dissolves 15-20min；
Zinc acetate solution is cooled to 50 DEG C of water-baths, dispersant is added therewith, 20-25min is stirred, hydroxide is then added
Sodium solution reacts 15min in 50 DEG C of water-baths, obtains nano oxidized zinc solution；
Wherein, zinc acetate solution, sodium hydroxide solution, dispersant volume ratio be 20：20：1；
The preparation of S2, nano zine oxide core-shell quanta dots solution
It pipettes in concentrated ammonia liquor to ethanol solution and is diluted, ultrasonic mixing is uniform, obtains ammonium hydroxide dilution, is subsequently placed in appearance
It is preserved in measuring bottle for use；
Wherein, the volume ratio of concentrated ammonia liquor and ethyl alcohol is 1：500；
Nano oxidized zinc solution obtained in step S1 is cooled to 37 DEG C, be added dropwise in stirring water, ethyl orthosilicate,
Ammonium hydroxide dilution, 37 DEG C are stirred to react 60-70min, nano zine oxide core-shell quanta dots solution are made, and in 4 DEG C of preservations；
Wherein, the volume and prepare the vinegar being added when nano oxidized zinc solution that water, ethyl orthosilicate, ammonium hydroxide dilution are added
The volume ratio of sour zinc solution is 10：1：25：125；
The preparation of S3, nano zine oxide core-shell quanta dots
Nano zine oxide core-shell quanta dots solution obtained is centrifuged, is washed with ethyl alcohol and removes unreacted ion,
Product after washing is taken out, is dried at being 100 DEG C in temperature, obtains nano zine oxide core-shell quanta dots.
In the preparation process of nano oxidized zinc solution, solvent used is ethyl alcohol.
In the preparation process of nano oxidized zinc solution, dispersant used is polyethylene glycol 200.
In the preparation process of nano zine oxide core-shell quanta dots solution, the water of addition is secondary water.
In the preparation process of nano oxidized zinc solution, used in stirring in water bath is DF-101S heat collecting type heated at constant temperature magnetic force
Blender.
The beneficial effects of the invention are as follows：The present invention is prepared for the zinc oxide of nucleocapsid using a kind of simple mild method
Core-shell quanta dots, condition requirement is low, using ethyl alcohol as solvent, using polyethylene glycol 200 as dispersion stabilizer, and the nano-particle of preparation
The smaller and good dispersion of grain, particle distribution is uniform, is suitble to large-scale industrial production；The ultraviolet screen of Zinc oxide quantum dot of preparation
It covers effect and the transparency is good, there is application prospect.
Specific implementation mode
The present invention is further explained in the light of specific embodiments：
A kind of preparation method of nano zine oxide core-shell quanta dots, the specific steps are：
The preparation of S1, nano oxidized zinc solution
It weighs Zinc diacetate dihydrate to be dissolved in solvent, is configured to the zinc acetate solution of a concentration of 0.1mol/L, weighs hydrogen-oxygen
Change sodium to be dissolved in solvent, is configured to the sodium hydroxide solution of a concentration of 0.1mol/L；
Stirred in water bath by prepared zinc acetate solution at 55 DEG C -60 DEG C dissolves 30-40min；
Stirred in water bath by prepared sodium hydroxide solution at 50 DEG C dissolves 15-20min；
Zinc acetate solution is cooled to 50 DEG C of water-baths, dispersant is added therewith, 20-25min is stirred, hydroxide is then added
Sodium solution reacts 15min in 50 DEG C of water-baths, obtains nano oxidized zinc solution；
Wherein, zinc acetate solution, sodium hydroxide solution, dispersant volume ratio be 20：20：1；
The preparation of S2, nano zine oxide core-shell quanta dots solution
It pipettes in concentrated ammonia liquor to ethanol solution and is diluted, ultrasonic mixing is uniform, obtains ammonium hydroxide dilution, is subsequently placed in appearance
It is preserved in measuring bottle for use；
Wherein, the volume ratio of concentrated ammonia liquor and ethyl alcohol is 1：500；
Nano oxidized zinc solution obtained in step S1 is cooled to 37 DEG C, be added dropwise in stirring water, ethyl orthosilicate,
Ammonium hydroxide dilution, 37 DEG C are stirred to react 60-70min, nano zine oxide core-shell quanta dots solution are made, and in 4 DEG C of preservations；
Wherein, the volume and prepare the vinegar being added when nano oxidized zinc solution that water, ethyl orthosilicate, ammonium hydroxide dilution are added
The volume ratio of sour zinc solution is 10：1：25：125；
The preparation of S3, nano zine oxide core-shell quanta dots
Nano zine oxide core-shell quanta dots solution obtained is centrifuged, is washed with ethyl alcohol and removes unreacted ion,
Product after washing is taken out, is dried at being 100 DEG C in temperature, obtains nano zine oxide core-shell quanta dots.
In the preparation process of nano oxidized zinc solution, solvent used is ethyl alcohol.
In the preparation process of nano oxidized zinc solution, dispersant used is polyethylene glycol 200.
In the preparation process of nano zine oxide core-shell quanta dots solution, the water of addition is secondary water.
In the preparation process of nano oxidized zinc solution, used in stirring in water bath is DF-101S heat collecting type heated at constant temperature magnetic force
Blender.
Specific embodiment 1：
A kind of preparation method of nano zine oxide core-shell quanta dots, the specific steps are：
The preparation of S1, nano oxidized zinc solution
It weighs Zinc diacetate dihydrate to be dissolved in solvent, is configured to the zinc acetate solution of a concentration of 0.1mol/L, weighs hydrogen-oxygen
Change sodium to be dissolved in solvent, is configured to the sodium hydroxide solution of a concentration of 0.1mol/L；
Stirred in water bath by prepared zinc acetate solution at 55 DEG C dissolves 30min；
Stirred in water bath by prepared sodium hydroxide solution at 50 DEG C dissolves 15min；
Zinc acetate solution is cooled to 50 DEG C of water-baths, dispersant is added therewith, 25min is stirred, sodium hydroxide is then added
Solution reacts 15min in 50 DEG C of water-baths, obtains nano oxidized zinc solution；
Wherein, zinc acetate solution, sodium hydroxide solution, dispersant volume ratio be 20：20：1；
The preparation of S2, nano zine oxide core-shell quanta dots solution
It pipettes in concentrated ammonia liquor to ethanol solution and is diluted, ultrasonic mixing is uniform, obtains ammonium hydroxide dilution, is subsequently placed in appearance
It is preserved in measuring bottle for use；
Wherein, the volume ratio of concentrated ammonia liquor and ethyl alcohol is 1：500；
Nano oxidized zinc solution obtained in step S1 is cooled to 37 DEG C, be added dropwise in stirring water, ethyl orthosilicate,
Ammonium hydroxide dilution, 37 DEG C are stirred to react 60min, nano zine oxide core-shell quanta dots solution are made, and in 4 DEG C of preservations；
Wherein, the volume and prepare the vinegar being added when nano oxidized zinc solution that water, ethyl orthosilicate, ammonium hydroxide dilution are added
The volume ratio of sour zinc solution is 10：1：25：125；
The preparation of S3, nano zine oxide core-shell quanta dots
Nano zine oxide core-shell quanta dots solution obtained is centrifuged, is washed with ethyl alcohol and removes unreacted ion,
Product after washing is taken out, is dried at being 100 DEG C in temperature, obtains nano zine oxide core-shell quanta dots.
In the preparation process of nano oxidized zinc solution, solvent used is ethyl alcohol.
In the preparation process of nano oxidized zinc solution, dispersant used is polyethylene glycol 200.
In the preparation process of nano zine oxide core-shell quanta dots solution, the water of addition is secondary water.
In the preparation process of nano oxidized zinc solution, used in stirring in water bath is DF-101S heat collecting type heated at constant temperature magnetic force
Blender.
Specific embodiment 2：
A kind of preparation method of nano zine oxide core-shell quanta dots, the specific steps are：
The preparation of S1, nano oxidized zinc solution
It weighs Zinc diacetate dihydrate to be dissolved in solvent, is configured to the zinc acetate solution of a concentration of 0.1mol/L, weighs hydrogen-oxygen
Change sodium to be dissolved in solvent, is configured to the sodium hydroxide solution of a concentration of 0.1mol/L；
Stirred in water bath by prepared zinc acetate solution at 60 DEG C dissolves 40min；
Stirred in water bath by prepared sodium hydroxide solution at 50 DEG C dissolves 20min；
Zinc acetate solution is cooled to 50 DEG C of water-baths, dispersant is added therewith, 20min is stirred, sodium hydroxide is then added
Solution reacts 15min in 50 DEG C of water-baths, obtains nano oxidized zinc solution；
Wherein, zinc acetate solution, sodium hydroxide solution, dispersant volume ratio be 20：20：1；
The preparation of S2, nano zine oxide core-shell quanta dots solution
It pipettes in concentrated ammonia liquor to ethanol solution and is diluted, ultrasonic mixing is uniform, obtains ammonium hydroxide dilution, is subsequently placed in appearance
It is preserved in measuring bottle for use；
Wherein, the volume ratio of concentrated ammonia liquor and ethyl alcohol is 1：500；
Nano oxidized zinc solution obtained in step S1 is cooled to 37 DEG C, be added dropwise in stirring water, ethyl orthosilicate,
Ammonium hydroxide dilution, 37 DEG C are stirred to react 70min, nano zine oxide core-shell quanta dots solution are made, and in 4 DEG C of preservations；
Wherein, the volume and prepare the vinegar being added when nano oxidized zinc solution that water, ethyl orthosilicate, ammonium hydroxide dilution are added
The volume ratio of sour zinc solution is 10：1：25：125；
The preparation of S3, nano zine oxide core-shell quanta dots
Nano zine oxide core-shell quanta dots solution obtained is centrifuged, is washed with ethyl alcohol and removes unreacted ion,
Product after washing is taken out, is dried at being 100 DEG C in temperature, obtains nano zine oxide core-shell quanta dots.
In the preparation process of nano oxidized zinc solution, solvent used is ethyl alcohol.
In the preparation process of nano oxidized zinc solution, dispersant used is polyethylene glycol 200.
In the preparation process of nano zine oxide core-shell quanta dots solution, the water of addition is secondary water.
In the preparation process of nano oxidized zinc solution, used in stirring in water bath is DF-101S heat collecting type heated at constant temperature magnetic force
Blender.
Specific embodiment 3：
A kind of preparation method of nano zine oxide core-shell quanta dots, the specific steps are：
The preparation of S1, nano oxidized zinc solution
It weighs Zinc diacetate dihydrate to be dissolved in solvent, is configured to the zinc acetate solution of a concentration of 0.1mol/L, weighs hydrogen-oxygen
Change sodium to be dissolved in solvent, is configured to the sodium hydroxide solution of a concentration of 0.1mol/L；
Stirred in water bath by prepared zinc acetate solution at 58 DEG C dissolves 35min；
Stirred in water bath by prepared sodium hydroxide solution at 50 DEG C dissolves 18min；
Zinc acetate solution is cooled to 50 DEG C of water-baths, dispersant is added therewith, 22min is stirred, sodium hydroxide is then added
Solution reacts 15min in 50 DEG C of water-baths, obtains nano oxidized zinc solution；
Wherein, zinc acetate solution, sodium hydroxide solution, dispersant volume ratio be 20：20：1；
The preparation of S2, nano zine oxide core-shell quanta dots solution
It pipettes in concentrated ammonia liquor to ethanol solution and is diluted, ultrasonic mixing is uniform, obtains ammonium hydroxide dilution, is subsequently placed in appearance
It is preserved in measuring bottle for use；
Wherein, the volume ratio of concentrated ammonia liquor and ethyl alcohol is 1：500；
Nano oxidized zinc solution obtained in step S1 is cooled to 37 DEG C, be added dropwise in stirring water, ethyl orthosilicate,
Ammonium hydroxide dilution, 37 DEG C are stirred to react 65min, nano zine oxide core-shell quanta dots solution are made, and in 4 DEG C of preservations；
Wherein, the volume and prepare the vinegar being added when nano oxidized zinc solution that water, ethyl orthosilicate, ammonium hydroxide dilution are added
The volume ratio of sour zinc solution is 10：1：25：125；
The preparation of S3, nano zine oxide core-shell quanta dots
Nano zine oxide core-shell quanta dots solution obtained is centrifuged, is washed with ethyl alcohol and removes unreacted ion,
Product after washing is taken out, is dried at being 100 DEG C in temperature, obtains nano zine oxide core-shell quanta dots.
In the preparation process of nano oxidized zinc solution, solvent used is ethyl alcohol.
In the preparation process of nano oxidized zinc solution, dispersant used is polyethylene glycol 200.
In the preparation process of nano zine oxide core-shell quanta dots solution, the water of addition is secondary water.
In the preparation process of nano oxidized zinc solution, used in stirring in water bath is DF-101S heat collecting type heated at constant temperature magnetic force
Blender.
The present invention is prepared for the zinc oxide core-shell quanta dots of nucleocapsid, condition requirement using a kind of simple mild method
Low, using ethyl alcohol as solvent, using polyethylene glycol 200 as dispersion stabilizer, the nano-particle particle of preparation is smaller and good dispersion, grain
Son is evenly distributed, and is suitble to large-scale industrial production；The ultraviolet shielded effect of Zinc oxide quantum dot and the transparency of preparation are good, tool
There is application prospect.
The present invention is exemplarily described above in conjunction with specific embodiment, it is clear that the present invention implements not by upper
The limitation of mode is stated, if the various improvement of inventive concept and technical scheme of the present invention progress are used, or it is not improved straight
It scoops out for other occasions, within protection scope of the present invention.
Claims (5)
1. a kind of preparation method of nano zine oxide core-shell quanta dots, which is characterized in that the specific steps are：
The preparation of S1, nano oxidized zinc solution
It weighs Zinc diacetate dihydrate to be dissolved in solvent, is configured to the zinc acetate solution of a concentration of 0.1mol/L, weighs sodium hydroxide
It is dissolved in solvent, is configured to the sodium hydroxide solution of a concentration of 0.1mol/L；
Stirred in water bath by prepared zinc acetate solution at 55 DEG C -60 DEG C dissolves 30-40min；
Stirred in water bath by prepared sodium hydroxide solution at 50 DEG C dissolves 15-20min；
Zinc acetate solution is cooled to 50 DEG C of water-baths, dispersant is added therewith, stirs 20-25min, it is molten that sodium hydroxide is then added
Liquid reacts 15min in 50 DEG C of water-baths, obtains nano oxidized zinc solution；
Wherein, zinc acetate solution, sodium hydroxide solution, dispersant volume ratio be 20：20：1；
The preparation of S2, nano zine oxide core-shell quanta dots solution
It pipettes in concentrated ammonia liquor to ethanol solution and is diluted, ultrasonic mixing is uniform, obtains ammonium hydroxide dilution, is subsequently placed in volumetric flask
It is middle to preserve for use；
Wherein, the volume ratio of concentrated ammonia liquor and ethyl alcohol is 1：500；
Nano oxidized zinc solution obtained in step S1 is cooled to 37 DEG C, water, ethyl orthosilicate, ammonium hydroxide are added dropwise in stirring
Dilution, 37 DEG C are stirred to react 60-70min, nano zine oxide core-shell quanta dots solution are made, and in 4 DEG C of preservations；
Wherein, the volume and prepare the zinc acetate being added when nano oxidized zinc solution that water, ethyl orthosilicate, ammonium hydroxide dilution are added
The volume ratio of solution is 10：1：25：125；
The preparation of S3, nano zine oxide core-shell quanta dots
Nano zine oxide core-shell quanta dots solution obtained is centrifuged, is washed with ethyl alcohol and removes unreacted ion, will washed
Product after washing takes out, and is dried at being 100 DEG C in temperature, obtains nano zine oxide core-shell quanta dots.
2. a kind of preparation method of nano zine oxide core-shell quanta dots according to claim 1, which is characterized in that nano oxygen
In the preparation process for changing zinc solution, solvent used is ethyl alcohol.
3. a kind of preparation method of nano zine oxide core-shell quanta dots according to claim 2, which is characterized in that nano oxygen
In the preparation process for changing zinc solution, dispersant used is polyethylene glycol 200.
4. a kind of preparation method of nano zine oxide core-shell quanta dots according to claim 3, which is characterized in that nano oxygen
In the preparation process for changing zinc core-shell quanta dots solution, the water of addition is secondary water.
5. a kind of preparation method of nano zine oxide core-shell quanta dots according to claim 4, which is characterized in that nano oxygen
In the preparation process for changing zinc solution, used in stirring in water bath is DF-101S heat collecting type constant-temperature heating magnetic stirring apparatus.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110563023A (en) * | 2019-09-23 | 2019-12-13 | 陕西科技大学 | high-fluorescence-brightness ZnO quantum dot and preparation method thereof |
| CN111205578A (en) * | 2018-11-22 | 2020-05-29 | 深圳光启超材料技术有限公司 | Ultraviolet absorbing film and method for producing the same |
-
2018
- 2018-05-17 CN CN201810472339.XA patent/CN108517206A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111205578A (en) * | 2018-11-22 | 2020-05-29 | 深圳光启超材料技术有限公司 | Ultraviolet absorbing film and method for producing the same |
| CN111205578B (en) * | 2018-11-22 | 2022-11-08 | 深圳光启超材料技术有限公司 | Ultraviolet absorbing film and method for producing the same |
| CN110563023A (en) * | 2019-09-23 | 2019-12-13 | 陕西科技大学 | high-fluorescence-brightness ZnO quantum dot and preparation method thereof |
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